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开发用于分析消费品中痕量全氟烷基醇排放的热解吸-气相色谱-串联质谱(TD-GC-MS/MS)分析方法。

Method development for thermal desorption-gas chromatography-tandem mass spectrometry (TD-GC-MS/MS) analysis of trace level fluorotelomer alcohols emitted from consumer products.

机构信息

Oak Ridge Institute for Science and Education Postdoctoral Fellow at U.S. Environmental Protection Agency, Office of Research and Development, Center for Environmental Measurement and Modeling, Research Triangle Park, NC 27711, United States.

U.S. Environmental Protection Agency, Office of Research and Development, Center for Environmental Measurement and Modeling, Research Triangle Park, NC 27711, United States.

出版信息

J Chromatogr A. 2023 Aug 30;1705:464204. doi: 10.1016/j.chroma.2023.464204. Epub 2023 Jul 6.

Abstract

The scientific foundation for per- and polyfluoroalkyl substances (PFAS) measurements in water, soils, sediments, biosolids, biota, and outdoor air has rapidly expanded; however, there are limited efforts devoted to developing analytical methods to measure vapor-phase PFAS in indoor air. A gas chromatography-tandem mass spectrometry (GC-MS/MS) method coupled with thermal desorption (TD) sorbent tube analysis was developed to quantify trace levels of fluorotelomer alcohols (FTOHs) emitted from consumer products in the indoor environment. Method evaluation included determination of instrument detection limits (IDLs), quality assurance checks of target standards purchased from different vendors, sample loss during storage, and TD sorbent breakthrough with tubes coupled in-series. The IDLs for TD-GC-MS/MS analyses ranged from 0.07 - 0.09 ng/tube. No significant loss of FTOHs was observed during stability tests over 28 days with relative standard deviations (RSDs) of spiked TD tubes ranging from 3.1 - 7.7% and the RSDs of polypropylene copolymer vial storage of standard solutions ranging from 4.3 - 8.4%. TD tube breakthrough was minimal with recovered FTOHs in the second tubes <1% of the spiked concentrations in the first tubes with carrier gas volume up to 20 L. The method has been applied to determine FTOH emissions from three consumer products in micro-scale chambers. A liquid stone cleaner/sealer product contained the highest levels of 6:2, 8:2, and 10:2 FTOHs, while the mattress pad products contained lower levels of 8:2 and 10:2 FTOHs. The emission parameters, including the initial emission factors and first order decay rate constants, were obtained based on the experimental data. The developed methods are sensitive and specific for analysis of all four target FTOHs (4:2, 6:2, 8:2, 10:2 FTOHs) with chamber testing. The methods can be extended to indoor air sampling and could be applicable to ambient air sampling.

摘要

全氟和多氟烷基物质(PFAS)在水中、土壤、沉积物、生物固体、生物群和室外空气中的测量的科学基础已经迅速扩展;然而,用于测量室内空气中气相 PFAS 的分析方法的开发工作有限。建立了一种气相色谱-串联质谱(GC-MS/MS)方法,结合热解吸(TD)吸附管分析,用于量化室内环境中来自消费产品的氟调聚物醇(FTOH)的痕量排放。方法评估包括仪器检测限(IDL)的确定、从不同供应商购买的目标标准的质量保证检查、储存过程中的样品损失以及串联耦合的 TD 吸附管的穿透。TD-GC-MS/MS 分析的 IDL 范围为 0.07-0.09ng/管。在 28 天的稳定性测试中,未观察到 FTOH 明显损失,带有 TD 管的加标管的相对标准偏差(RSD)范围为 3.1-7.7%,标准溶液的聚丙烯共聚物小瓶储存的 RSD 范围为 4.3-8.4%。当载气体积高达 20L 时,第二管中回收的 FTOH 小于第一管中加标浓度的 1%,TD 管穿透最小。该方法已应用于在微尺度腔室中确定三种消费品的 FTOH 排放。一种液体石材清洁剂/密封剂产品含有最高水平的 6:2、8:2 和 10:2 FTOH,而床垫垫产品则含有较低水平的 8:2 和 10:2 FTOH。根据实验数据获得了排放参数,包括初始排放因子和一阶衰减速率常数。所开发的方法对于所有四种目标 FTOH(4:2、6:2、8:2、10:2 FTOH)的腔室测试具有灵敏性和特异性。该方法可以扩展到室内空气采样,也可适用于环境空气采样。

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